Abstract 3,4-Methylenedioxymethamphetamine (MDMA) is a popular illicit drug. Given its adverse effects, the growing abuse of MDMA worldwide, and the need for forensic chemistry methods that minimize environmental issues, here we report a green approach for quantitative MDMA analysis in ecstasy tablets based on phenyl reversed-phase liquid-chromatography coupled to a diode-array detector. Water with 0.1% formic acid (pH adjusted to 5.00 with ammonium hydroxide) and ethanol (85:15, v/v) was employed as the mobile phase. The method showed good analytical performance in terms of linearity (0.0031–0.1 mg mL−1, R 2 = 0.9998), precision (1.26–7.79%), accuracy (93.5–107.7%), and recovery (96.6–100.6%). The limits of detection and quantification were 0.0007 and 0.0031 mg mL−1, respectively. The MDMA purity ranged from 14.7% to 35.1% (m/m). Additionally, greenness assessment using an eco-scale metric provided a score. The results indicated that the simultaneous use of ethanol and phenyl-bonded phase provides high selectivity and is suitable and reliable for routine analysis of seized ecstasy samples, constituting a powerful alternative to expensive mass spectrometer-based liquid chromatography and common reversed-phase columns. Graphical Abstract

中文翻译：

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经验证的绿色苯基反相 LC 方法使用乙醇测定缉获的摇头丸中的 MDMA

摘要 3,4-亚甲二氧基甲基苯丙胺 (MDMA) 是一种流行的非法药物。鉴于 MDMA 的不利影响、世界范围内 MDMA 的日益滥用以及对尽量减少环境问题的法医化学方法的需求，我们在这里报告了一种基于苯基反相液相色谱与二极管耦合的摇头丸中 MDMA 定量分析的绿色方法-阵列检测器。使用含有 0.1% 甲酸（用氢氧化铵将 pH 值调节至 5.00）和乙醇 (85:15, v/v) 的水作为流动相。该方法在线性 (0.0031–0.1 mg mL-1, R 2 = 0.9998)、精密度 (1.26–7.79%)、准确度 (93.5–107.7%) 和回收率 (96.6–100.6%) 方面显示出良好的分析性能。检测限和定量限分别为 0.0007 和 0.0031 mg mL-1。MDMA 纯度范围从 14.7% 到 35.1% (m/m)。此外，使用生态尺度指标进行的绿色评估提供了一个分数。结果表明，同时使用乙醇和苯基键合相提供了高选择性，适用于缉获的摇头丸样品的常规分析，是可靠的，是昂贵的基于质谱仪的液相色谱和常见反相柱的有力替代品。图形概要